CN110511755A - A kind of indigo plant is light activated to mix the molybdate red luminescent material of Mn4+ - Google Patents
A kind of indigo plant is light activated to mix the molybdate red luminescent material of Mn4+ Download PDFInfo
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- CN110511755A CN110511755A CN201910852696.3A CN201910852696A CN110511755A CN 110511755 A CN110511755 A CN 110511755A CN 201910852696 A CN201910852696 A CN 201910852696A CN 110511755 A CN110511755 A CN 110511755A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
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Abstract
The present invention relates to inorganic functional material field, disclose that a kind of indigo plant is light activated to mix Mn4+Molybdate red luminescent material and its synthetic method.Indigo plant of the invention is light activated to mix Mn4+Molybdate red luminescent material chemical composition be K2(Mo1‑xO2F4)H2O:xMn4+；X is corresponding doping Mn4+Ion is with respect to Mo6+Molar percentage coefficient shared by ion, 0 < x≤0.20.Red illuminating material according to the present invention is under blue light excitation, and based on the red emission of 627 nm or so, luminous efficiency is high.Indigo plant according to the present invention is light activated to mix Mn4+Molybdate red luminescent material preparation method be liquid phase method, carry out at normal temperature, synthesis technology is simple, be suitble to large-scale industrial production.
Description
Technical field
Mn is mixed the present invention relates to a kind of indigo plant is light activated4+Molybdate red luminescent material and preparation method thereof, belong to nothing
Machine functional material synthesizes field.
Background technique
In the lighting system in the present age, core component of the fluorescent powder as white light-emitting diodes (LED), because it is with efficiency
The advantages that height, service life length, energy-saving and environmental protection, it is widely used in illuminating.But such fluorescent powder causes due to lacking red component
Many disadvantages such as its colour temperature is higher, and colour rendering index is low, are not particularly suited for room lighting.It is most of red using fluoride as matrix
Color luminescent material, there are many its activator type, such as Mn4+、Mn2+Deng.It is doped with Mn4+Red fluorescence powder, low in cost, ring
It protects pollution-free, emits strong peak in red light district, compensate for that red fluorescence powder property currently on the market is unstable, low bad of luminous efficiency
Gesture.And the characteristics of fluoride low phonon energy, can reduce the quenching of ion excited state, improve the luminous efficiency of substance.
With blue light GaN chip excitated red fluorescent powder, colour temperature can be reduced, improves colour rendering index.Studies have shown that Mn4+In
Under the excitation of blue light GaN chip, high-intensitive red emission peak can be generated.Mn4+The red fluorescence powder of doping has stability height,
The features such as coloration is high, and light decay is small, with Mn4+The red fluorescence powder for doing Doped ions is applied to LED, it will can be greatly reduced glimmering at present
The high cost of light powder, potential meaning and value will be had by improving LED performance.
In this invention, we report successfully develops what novel blue light effectively excited in a solution of hydrofluoric acid
Mn4+The molybdate red luminescent material K of activation2(Mo1-xO2F4)H2O:xMn4+(x is corresponding doping Mn4+Ion is with respect to Mo6+Ion
Shared molar percentage coefficient, 0 < x≤0.20) and preparation method thereof.
Summary of the invention
Mn is mixed the object of the present invention is to provide a kind of indigo plant is light activated4+Molybdate red luminescent material.
It is a further object to provide the preparation methods of above-mentioned red illuminating material.
To achieve the goals above, indigo plant according to the present invention is light activated mixes Mn4+Molybdate red luminescent material,
Chemical composition are as follows: K2(Mo1-xO2F4)H2O:xMn4+；X is corresponding doping Mn4+Ion is with respect to Mo6+Molar percentage shared by ion
Coefficient, 0 < x≤0.20.The mass percentage of raw material type used in the present invention and each raw material is respectively as follows: potassium fluoride:
31.0~ 34.0 %；Potassium hexafluoromanganate: 2.5 ~ 20.0 %；Ammonium molybdate: 47.0 ~ 52.0 %；Hydrofluoric acid: 21.0 ~ 24.0 %.
Blue light wavelength of the present invention is 440~490 nm.
The preparation method of above-mentioned red illuminating material is using liquid phase method, and various raw materials are by above-mentioned stoichiometric ratio.Tool
Body, which includes the following steps: that first ammonium molybdate and potassium hexafluoromanganate are added in hydrofluoric acid solution, to be stirred 30~60 minutes, has directly been dissolved
Entirely, potassium fluoride is then added and continues stirring 2~6 hours.Gained sediment dehydrated alcohol and glacial acetic acid respectively wash 3 times, finally in
24 hours dry in vacuum oven, obtained orange red powder is final products.
Red illuminating material of the invention shows very strong red emission under blue light excitation, and (emission peak is located at 627 nm
Left and right), luminous efficiency is high.
Detailed description of the invention
Fig. 1 is K in example 12(MoO2F4)H2O:Mn4+XRD diffraction pattern；
Fig. 2 is K in example 12(MoO2F4)H2O:Mn4+Scanning electron microscopic picture；
Fig. 3 is K in example 12(MoO2F4)H2O:Mn4+Room temperature excitation spectrum (monitoring wavelength be 627 nm) and emission spectrum it is (sharp
Hair wavelength is 471 nm)；
Fig. 4 is K in example 12(MoO2F4)H2O:Mn4+With commercial YAG:Ce3+Made by yellow fluorescent powder and blue-light LED chip
Warm white LED device 20 mA electric currents excitation under electroluminescent light spectrogram.
Specific embodiment
Embodiment 1:
It weighs 7.25 grams of ammonium molybdates and 0.62 gram of potassium hexafluoromanganate is dissolved in 50ml hydrofluoric acid (40wt%), 60 points are stirred under room temperature
Clock adds 34.76 grams of fluorinations nak response 3 hours into this solution to dissolving completely.Gained sediment dehydrated alcohol and ice
Acetic acid is respectively washed 3 times, is finally dried 24 hours in a vacuum drying oven, and obtained orange red powder is final products K2(MoO2F4)
H2O:Mn4+。
The XRD diffraction pattern of this fluorescent powder is as shown in Fig. 1, the diffraction maximum and matrix K of sample2(MoO2F4)H2O standard card
JCPDS 73-2350 is completely the same, and the diffraction maximum of any miscellaneous phase is not observed, this shows the sample purity synthesized by us
Height is anorthic crystal structure.
Fig. 2 show K2(MoO2F4)H2O:Mn4+Scanning electron microscopic picture, sample particle is club shaped structure, be about 25 μm,
About 1-2 μm of diameter.
(excitation wavelength is the room temperature excitation spectrum (monitoring wavelength be 627 nm) and emission spectrum that attached drawing 3 show sample
471 nm).Sample is all shown very in ultraviolet region (nm of 320 nm ~ 390) and blue light area (nm of 400 nm ~ 500)
Strong broadband excitation, most strong excitation peak are located at 471 nm or so.Under the blue light excitation of 471 nm, being emitted as sample is a series of
Spike, most strong emission peak is in 627 nm or so.Spectrum CIE coordinate value are as follows:x=0.376, y=0.354。
Fig. 4 show K2(MoO2F4)H2O:Mn4+With commercial YAG:Ce3+Made by yellow fluorescent powder and blue-light LED chip
Warm white LED device 20 mA electric currents excitation under electroluminescent light spectrogram.The blue light emission peak of 460 nm originates from figure
The emission peak of the transmitting of GaN chip, 500 nm to 600 nm ranges originates from YAG:Ce3+Yellow emission.The hair of our samples
It penetrates and is located at red light region, most strong transmitting is located at 627 nm.This warm white LED colour temperature is low, and colour rendering index is high.
Embodiment 2:
It weighs 7.73 grams of ammonium molybdates and 0.31 gram of potassium hexafluoromanganate is dissolved in 40 ml hydrofluoric acid (40 wt%), stir 50 under room temperature
Minute to dissolving completely, 34.86 grams of potassium fluorides is added into this solution and are reacted 4 hours.Gained sediment dehydrated alcohol
It respectively washes with glacial acetic acid 3 times, finally dries 24 hours in a vacuum drying oven, obtained orange red powder is final products K2
(MoO2F4)H2O:Mn4+。
Embodiment 3:
It weighs 7.25 grams of ammonium molybdates and 0.62 gram of potassium hexafluoromanganate is dissolved in 40 ml hydrofluoric acid (40 wt%), stir 60 under room temperature
Minute, to dissolving completely, 34.86 grams of fluorinations nak response 6 hours were added into this solution.Gained sediment dehydrated alcohol and
Glacial acetic acid is respectively washed 3 times, is finally dried 24 hours in a vacuum drying oven, and obtained orange red powder is final products K2
(MoO2F4)H2O:Mn4+。
Claims (4)
1. a kind of indigo plant is light activated to mix Mn4+Molybdate red luminescent material, chemical composition are as follows: K2(Mo1-xO2F4)H2O:xMn4 +；X is corresponding doping Mn4+Ion is with respect to Mo6+Molar percentage coefficient shared by ion, 0 < x≤0.20.
2. indigo plant as described in claim 1 is light activated to mix Mn4+Molybdate red luminescent material, it is characterised in that the blue light
Refer to that wavelength is the light of 420~480 nm.
3. indigo plant as described in claim 1 is light activated to mix Mn4+Molybdate red luminescent material preparation method, feature exists
It is liquid phase method in preparation method, includes the following steps: that first ammonium molybdate and potassium hexafluoromanganate are added in hydrofluoric acid solution and stir 30
~60 minutes, straight dissolution completely, was then added potassium fluoride and continues stirring 2~6 hours；Gained sediment dehydrated alcohol and ice vinegar
Acid is respectively washed 3 times, is finally dried 24 hours in a vacuum drying oven, and obtained orange red powder is final products.
4. indigo plant as claimed in claim 3 is light activated to mix Mn4+Molybdate red luminescent material preparation method, feature exists
It is respectively as follows: potassium fluoride: 31.0 ~ 34.0 % in the type of used raw material and the mass percentage of each raw material；Hexafluoro mangaic acid
Potassium: 2.5 ~ 20.0 %；Ammonium molybdate: 47.0 ~ 52.0 %；Hydrofluoric acid: 21.0 ~ 24.0 %.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410030A (en) * | 2020-12-03 | 2021-02-26 | 重庆文理学院 | Preparation method of multiphase composite molybdate oxyfluoride nano fluorescent material |
| JP2023526767A (en) * | 2020-04-22 | 2023-06-23 | エイエムエス－オスラム インターナショナル ゲーエムベーハー | Phosphor, method for manufacturing phosphor, and radiation-emitting device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800930A (en) * | 2017-01-10 | 2017-06-06 | 陕西师范大学 | A kind of oxyfluoride red fluorescence powder of Mn (IV) activation and preparation method thereof |
| CN110184057A (en) * | 2019-06-12 | 2019-08-30 | 上海应用技术大学 | A kind of oxygen fluoride red fluorescence powder and preparation method thereof |
-
2019
- 2019-09-10 CN CN201910852696.3A patent/CN110511755A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800930A (en) * | 2017-01-10 | 2017-06-06 | 陕西师范大学 | A kind of oxyfluoride red fluorescence powder of Mn (IV) activation and preparation method thereof |
| CN110184057A (en) * | 2019-06-12 | 2019-08-30 | 上海应用技术大学 | A kind of oxygen fluoride red fluorescence powder and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2023526767A (en) * | 2020-04-22 | 2023-06-23 | エイエムエス－オスラム インターナショナル ゲーエムベーハー | Phosphor, method for manufacturing phosphor, and radiation-emitting device |
| JP7482252B2 (en) | 2020-04-22 | 2024-05-13 | エイエムエス－オスラム インターナショナル ゲーエムベーハー | Phosphor, method for producing phosphor and radiation-emitting device |
| CN112410030A (en) * | 2020-12-03 | 2021-02-26 | 重庆文理学院 | Preparation method of multiphase composite molybdate oxyfluoride nano fluorescent material |
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